Instrumental Calibration, Standards, Quantitative Analysis, and ...

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Establishing Calibration of an Electron Microprobe • Wavelength spectrometer aligned vertically (baseplate) to coincide with optical microscope focal point in z-space • Diffracting crystal aligned to be on Roland circle • All WDS should focus on same z-axis and coincident xy area ~ 50 um in diameter • Characteristics of correct alignment All WDS & EDS have identical X-ray takeoff angle Maximum X-ray intensity at z focus position, but also require: Measure identical k-ratio within counting statistics • Simultaneous k-ratio measurement is ultimate test of alignment • Initial CMAS standard set used on Caltech MAC and JEOL JXA-733 • Expanded CMASTF standard set used for Wash U JXA-8200 UO EPMA Workshop 2008
Electron Microprobe Column Spectrometer Alignment: Baseplate and Crystal Baseplate: Place Rowland circle at Z focus Crystal: Align all crystals on Rowland circle Spectrometer design keeps detector on RC Note: Different K-ratio = misalignment Multiple spectrometer comparison required to demonstrate all WDS and EDS are mutually aligned UO EPMA Workshop 2008
Page 1 and 2: Electron-Probe Microanalysis: Instr
Page 3 and 4: Washington University, Saint Louis
Page 5 and 6: Pulse-Height Analysis Wavelength-di
Page 7 and 8: Detector Bias Scan Si Kα Vary Bias
Page 9 and 10: Calibration of PHA Using Bias vs. l
Page 11 and 12: Gain Shift Due to Count Rate 5K cps
Page 13 and 14: Carbon Kα PHA Scans Graphite, Fe3C
Page 15 and 16: WDS Deadtime Issues in EPMA • Dea
Page 17 and 18: Deadtime Losses Input - Output Curv
Page 19 and 20: Deadtime Relations Calculation of D
Page 21 and 22: Verification of Probe Current vs. A
Page 23 and 24: Deadtime Variation with Count Rate
Page 25: Alignment and Quantitative Analysis
Page 29 and 30: CMASTF Standard Inventory: Natural
Page 31 and 32: Ag Lα NIST SRM 481 AgAu Alloy (ψ=
Page 33 and 34: Historical CMAS Data Caltech MAC Pr
Page 35 and 36: Caltech JEOL 733 1990’s Spectrome
Page 37 and 38: Caltech JEOL 733 1990’s Spectrome
Page 39 and 40: Intercomparison of Measured vs. Acc
Page 41 and 42: WU JXA-8200 CMASTF Data Set Spectro
Page 47 and 48: Accuracy, 1σ % Error in K meas / K
Page 49 and 50: Washington University Earth and Pla
Page 51 and 52: Lunar Meteorite SAU169 Stage map 10
Page 53 and 54: WU8200 JEOL SDD 55 Fe Source Mn Kα
Page 55 and 56: SDD Performance Data: WU8200 SDD Mn
Page 57 and 58: WU8200 SDD Mn K Spectra T1, 100 sec
Page 59 and 60: WU8200 SDD Mn L Spectra T1, 100 sec
Page 61 and 62: WU8200 SDD Deadtime vs. Count Rate
Page 63 and 64: WU8200 SDD Count Rate vs. Resolutio
Page 65 and 66: Washington University JXA-8200 SDD
Page 67 and 68: CMASTF Standard Analyses WU8200 SDD
Page 69 and 70: CMASTF Standard Analyses WU8200 SDD
Page 71 and 72: EPMA Standards UO EPMA Workshop 200
Page 73 and 74: Basalt Glass Indian Ocean USNM 1137
Page 75 and 76: Olivine Standards: Mn, Fe, Ni Stand
Page 77 and 78:
Fayalite Standards Oxide MnO FeO* N
Page 79 and 80:
Systematic Error Using Oxide Standa
Page 81 and 82:
Accuracy of EPMA: Quantitative Anal
Page 83 and 84:
Olivine Alpha Factor Study: Compari
Page 85 and 86:
Analysis of Mg Kα in Shankland For
Page 87 and 88:
Mg Kα in Olivine Using Forsterite
Page 89 and 90:
EPMA of San Carlos Olivine Correcti
Page 91 and 92:
Inconel Spheres: Diameter ~ 30 um U
Page 93 and 94:
Inconel Sphere Low Energy EDS Regio
Page 95 and 96:
Al Kα Peak Intensity at -10º to +
Page 97 and 98:
Problem Systems UO EPMA Workshop 20
Page 99 and 100:
WDS Background Selection (Natural P
Page 101 and 102:
WDS Scan LIF: Al, Cr, Ni, and NiCrA
Page 103 and 104:
Zn Kα ΙΙ V Kα Ce Lα La Lα Ti
Page 105 and 106:
WDS Scan: PET Crystal 95IRV Green,
Page 107 and 108:
WDS Scan: PET Crystal Sr Lα Peaks,
Page 109 and 110:
Elevated and Uncertain MAC Values f
Page 111 and 112:
Mass Absorption Coefficients for Si
Page 113 and 114:
Silicon Kα MAC at L-edge of Absorb
Page 115 and 116:
Error Analysis Ta Lα in TaSi 2 All
Page 117 and 118:
Calculated Compositions of TaSi2 Re
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Instrumental Calibration, Standards, Quantitative Analysis, and ...

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